Proton Nuclear Magnetic Resonance Spectra Research Articles

Characterisation and critical processes identification for production of herbal preparations using 1H-NMR and chemometrics: A case study of Trichosanthis Pericarpium injection.

Herbal preparations are extensively utilised for the treatment of diseases in Asian countries. However, the variations in origin, climate, and production processes can lead to inconsistencies in the quality of herbal preparations. Existing quality control methods only target a few components in the finished product but ignore the control in the pharmaceutical process. Therefore, this study intends to develop a comprehensive component analysis method for intermediates in the pharmaceutical process to reveal the change patterns of substances and deepen the process understanding. This study aims to develop a rapid and comprehensive process characterisation and critical process identification method for herbal preparations. Six batches of Trichosanthis Pericarpium injection (TPI) intermediates were collected from the production process. Proton nuclear magnetic resonance (1H-NMR) spectra were acquired for qualitative and quantitative analysis of the se intermediates. Subsequently, chemometrics were used to identify critical processes and potential chemical markers. A total of 39 components in intermediates were identified, and the transfer of 25 components during the production process was investigated. Column chromatography was determined as the critical process. Nine components were identified as chemical markers. The application of 1H-NMR facilitated a comprehensive reflection of the chemical composition information of process intermediates, enabling investigations into the transfer of multi-component substances and accurate identification of critical processes and chemical markers.

Combining Siloxane-Based polybenzoxazine with Poly(ethylene-co-vinyl acetate/hydroxyl) for tougher, more Stable, and Self-Healable materials

Cross-linked EVOH containing dynamic silyl ether bonds with improved toughness and processability have been prepared by taking advantage of both ethylene vinyl alcohol (EVOH) and benzoxazine chemistry. For that, the cross-linked EVOH was synthesized through a trans etherification reaction between siloxane mono-functional benzoxazine and pendant hydroxyl groups on ethylene vinyl alcohol (EVOH) copolymer. The precursor EVOH copolymer was obtained by hydrolysis of the commercially available and inexpensive ethylene–vinyl acetate copolymer (EVA). The chemical structures of polymers were analyzed by proton nuclear magnetic resonance (1H NMR) spectra and Fourier transform infrared (FTIR) spectroscopy. The curing and thermal stability were researched by using differential scanning calorimetry (DSC) and a thermogravimetric analyzer (TGA), respectively. The mechanical properties via the stress–strain analysis were examined to identify the effect of the benzoxazines with the silyl ether group on the toughness and self-healing ability of the modified EVOH.

Thermal Stability of Protic Ionic Liquids.

While protic ionic liquids (ILs) have found great success as solvents for a broad range of applications, little is known about their degradation when exposed to temperatures above ambient for extended periods of time. Here, we report the thermal stability of six protic ILs, namely, ethylammonium nitrate, ethylammonium formate, ethylammonium acetate, ethanolammonium nitrate, ethanolammonium formate, and ethanolammonium acetate. The effect of heating each ionic liquid to 60 °C for 1 h or 1 week (sealed or open to the atmosphere) was evaluated by considering the changes to water content, pH, mass, thermal phase transitions, and molecular structure after each treatment. Heating each of the six ILs when sealed led to measurable shifts in their water content and 10 wt % pH, but there was no significant change in their mass, thermal phase transitions according to differential scanning calorimetry (DSC), or molecular structure using proton nuclear magnetic resonance (1H NMR) spectra, indicating that the samples were largely unchanged. The samples that were heated open to the atmosphere also displayed no significant changes after 1 h but displayed significant changes after 1 week.

Mechanisms of acrylamide biosorption by Lactobacillus plantarum ATCC8014 peptidoglycan

This study extracted peptidoglycan (PG) from Lactobacillus plantarum ATCC8014, its acrylamide (AA) adsorption behavior was evaluated by creating adsorption models, and its binding characterizations were investigated by physicochemical methods. The kinetics and isothermal model revealed that the biosorption of AA by PG conformed to Langmuir, Freundlich equations, and the second-order kinetic model, confirming that the adsorption process involved both physisorption and chemisorption. Fourier transform infrared spectroscopy and chemical blocking of functional groups confirmed that carboxyl, amino and hydroxyl groups were involved. Meanwhile, a new peak was generated in the proton nuclear magnetic resonance spectrum of PG upon adsorption, and the water contact angle was significantly reduced, indicating that hydrogen bonds and hydrophobic force were involved in the biosorption. Besides, energy dispersive spectroscopy and X-ray photoelectron spectroscopy results have important findings, suggesting that amide bonds might be formed during the adsorption process. Subsequently, this speculation was confirmed by the identification results of amidase. Overall, our results indicated that the mechanism of adsorption is complex and involves hydrogen bonding, hydrophobic forces and the formation of chemical bonds.

Construction and Single-Crystal Structures of N-Isoxazolin-5-ylcarbonylindole Derivatives, and Their Pesticidal Activities and Toxicology Study.

To explore natural product-based pesticide candidates, a series of indole derivatives containing the isoxazoline skeleton at the N-1 position were synthesized by 1,3-dipolar [2 + 3] cycloaddition reaction. Their structures were characterized by melting points (mp), infrared (IR) spectra, proton nuclear magnetic resonance spectra (1H NMR), carbon-13 nuclear magnetic resonance spectra (13C NMR), and high resolution mass spectrometry (HRMS). The single-crystal structures of five compounds were presented. Against Tetranychus cinnabarinus Boisduval, compound 3b showed greater than 3.8-fold acaricidal activity of indole and good control effects under glasshouse conditions. Against Aphis citricola Van der Goot, compounds 3b and 3q exhibited 48.3- and 36.8-fold aphicidal activity of indole and 6-methylindole, respectively. Particularly, compound 3b showed good bioactivities against T. cinnabarinus and A. citricola. Against Eriosoma lanigerum Hausmann, compound 3h and 3i showed 2.1 and 1.9 times higher aphicidal activity compared to indole. Furthermore, the construction of the epidermal cuticle layer of 3b-treated carmine spider mites was distinctly damaged, which ultimately led to their death.

Addition of Canna edulis starch and starch nanoparticles to stabilized Pickering emulsions: In vitro digestion and fecal fermentation

Starch nanoparticles (SNPs) were prepared through acid hydrolysis of Canna edulis native starch and modified with octenyl succinic anhydride (OSA) to yield OS-starch and OS-SNPs. These modified particles were used to stabilize curcumin-loaded Pickering emulsions. Effects on gut microbiota during in vitro fecal fermentation were examined. The surface of OS-starch exhibits a porous structure, while OS-SNPs display layered grooves. OSA modification was confirmed by Fourier transform infrared spectroscopy (with peaks at 1728 cm−1 and 1573 cm−1) and proton nuclear magnetic resonance spectra (0.5–2 ppm). The degree of substitution for OS-starch and OS-SNPs is 0.0106 ± 0.0004 and 0.0079 ± 0.0003, respectively. Following modification, the crystallinity decreased from 35.69 ± 0.46 % (native starch) to 30.17 ± 0.70 % (OS-starch), SNPs decreased from 45.87 ± 0.89 % to 43.63 ± 0.64 % (OS-SNPs). Contact angles for OS-starch and OS-SNPs are 77.47 ± 1.78 and 55.57 ± 0.21, respectively. OS-SNPs exhibited superior emulsification properties compared to OS-starch, forming stable Pickering emulsions with pseudoplastic fluid behavior and enhanced curcumin storage protection over 14 days (60.88 ± 4.26 %) with controlled release. Stabilizing Pickering emulsions with OS-starch and OS-SNPs positively affected on gut microbiota and improved the intestinal environment, showing promise for their application in transportation systems and innovative prebiotic food formulations.

Synthesis and pharmacological characterization of new curcumin ester pro-drugs with enhanced anti-inflammatory, anti-ulcerogenic and improved tissue distribution

In this work, curcumin- Non steroidal anti-inflammatory drugs (NSAIDs) conjugates were synthesized by esterification of the phenolic group of curcumin with the acid group of NSAIDs using the Steglich esterification method to enhance the anti-inflammatory activity of curcumin and to reduce the gastrointestinal side effects of NSAIDs. A set of bis C-NSAIDs conjugates was prepared by direct coupling of curcumin with Aceclofenac and Diflunisal respectively in good yield and characterized by Fourier-transform infrared spectra (FTIR) and Proton Nuclear Magnetic Resonance Spectra (1HNMR). In vivo, studies were performed to evaluate the toxicity, anti-inflammatory activity, bio-distribution, and anti-ulcerogenic studies of selected conjugates using different animal models. In Vivo, studies reveal enhanced biological activity with better tissue distribution of conjugates than that of parent curcumin and it could be a curcumin-based therapeutic molecule that might be explored further for its efficacy in managing inflammatory diseases.

Costa Rican Propolis Chemical Compositions: Nemorosone Found to Be Present in an Exclusive Geographical Zone.

The chemistry of Costa Rican propolis from Apis mellifera remains underexplored despite its potential applications. This study identified its chemical composition, linking chemotypes to antioxidant potential. Proton nuclear magnetic resonance (1H NMR) spectra were obtained for 119 propolis extracts and analyzed using multivariate analyses. In parallel, 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging assay was used to assess antioxidant activity. A generalized linear regression model (GLM) correlated this with its chemical profiles and geographical origin. Chromatographic methods were used to isolate active and inactive compounds, which were identified using nuclear magnetic resonance (NMR) and high-resolution mass spectrometry (HRMS). Principal component analysis (PCA) revealed three chemical profile groups for the 119 propolis extracts, explaining 73% of the total variance with two components. Radical scavenging activity was found to correlate with chemical composition. Isolation yielded n-coniferyl benzoate in type I (EC50 = 190 µg/mL, ORAC = 0.60 µmol TE/µmol) and nemorosone in type II (EC50 = 300 µg/mL, ORAC = 0.7 µmol TE/µmol). Type III was represented in terpene-like components, which exhibited lower antioxidant activity. This study categorizes Costa Rican propolis into three chemical types and identifies two key components linked to antioxidant activity. Notably, nemorosone, a valuable natural product, was found to be highly concentrated in a particular region of Costa Rica.

Re-Assemblable, Recyclable, and Self-Healing Epoxy Resin Adhesive Based on Dynamic Boronic Esters.

Thermosetting adhesives are commonly utilized in various applications. However, covalent cross-linked networks prevent thermosetting adhesives from being re-assembled, which necessitates higher machining precision. Additionally, the primary raw materials used in adhesive preparation are derived from non-renewable petroleum resources, which further constrain adhesive development. In this study, a recyclable adhesive was developed by incorporating dynamic boronic esters into epoxy resin derived from soybean oil. The successful synthesis of epoxidized soybean oil and boronic esters was confirmed through the analysis of proton nuclear magnetic resonance spectra and differential scanning calorimetry results. Swelling tests and tensile curves demonstrated the presence of covalently cross-linked networks. Self-healing and reprocessing experiments indicated that the cross-linked network topology could be re-assembled under mild conditions.

Reduction of the alcohol-stimulative taste of Japanese pot-distilled spirits

The Japanese traditional pot-distilled spirit shochu has various tastes that are produced by variations in the manufacturing processes. In this study, an alcohol-stimulative taste was organoleptically evaluated using shochu samples, and the chemical components and proton nuclear magnetic resonance (1H NMR) spectra were measured. In some shochu samples, the alcohol-stimulative taste was weaker than that of the standard 15% (v/v) EtOH-H2O mixture, and the water-ethanol hydrogen-bonding structure was stronger compared to a water-ethanol solution. However, some shochu samples filtered with ion-exchange resin had a strong alcohol-stimulative taste comparable to that of the standard 15% (v/v) EtOH-H2O mixture, and the hydrogen-bonding structure was found to be similar to that of the water-ethanol solution. We also investigated the effect of MgCl2 on reducing the alcohol-stimulative taste, and it was observed most strongly with in shochu samples filtered with ion-exchange resin. The change in chemical shift values of the 1H NMR spectra was also the largest in ion-exchange resin filtered shochu samples. The sensory reduction in the alcohol-stimulative taste could be enhanced by the strengthening of the water-ethanol hydrogen-bonding structure. Shochu samples contained many components in larger quantities compared to vodkas. It was found that MgCl2 could reduce the alcohol-stimulative taste of shochu samples. Some salts, such as MgCl2, can be introduced into spirits through the water used to dilute the ethanol content before bottling the products. Our results indicated that some components, such as MgCl2, present in water used can reduce the alcohol-stimulative taste of different spirits produced worldwide.

An AIPE-active fluorinated cationic Pt(II) complex for efficient detection of picric acid in aqueous media

A novel cationic Pt(II) complex 2 with 2-(2,4-difluorophenyl)pyridine as the cyclometalating ligand and 1,10-phenanthroline as the auxiliary ligand has been synthesized and fully characterized. This complex exhibits much higher aggregation-induced phosphorescent emission activity than that of a non-fluorinated complex 1 in CH3CN/H2O. The complex 2 demonstrates efficient detection on picric acid (PA) in CH3CN/H2O, providing a high quenching constant (KSV = 2.3 × 104 L/mol) and a low limit of detection (LOD = 0.26 µmol/L). In addition, complex 2 shows high selectivity for detection of PA in real water samples. Density functional theory calculations and proton nuclear magnetic resonance spectra suggest that the detection mechanism is attributed to the photo-induced electron transfer.

QBD APPROACH FOR THE DEVELOPMENT OF CAPSAICIN-LOADED STEARIC ACID-GRAFTED CHITOSAN POLYMERIC MICELLES

Objective: Capsaicin (CAP) is a naturally occurring alkaloid forecasted in the treatment of Alcoholic Hepatitis (AH), but least studied due to its hydrophobicity and low bioavailability. Hence, the present study aimed to optimize the parameters for the synthesis of stearic acid grafted chitosan (CS-g-SA) copolymer and preparation of CAP-loaded CS-g-SA micelles. Methods: Quality by design (QbD) approach in coordination with “Central composite designs (CCD) and Box–Behnken designs (BBD)” was used to optimize the process parameters. Results: CS-g-SA was synthesized at 80 °C, 480 min, and 946 rpm, at these optimized conditions, the average particle size and practical yield were found to be 134.70 nm and 85.69%, respectively. Proton Nuclear Magnetic Resonance (1H NMR) spectra depicted a sharp signal at d=1.0 ppm endorsing to -CH2 group of SA and confirming the formation of CS-g-SA copolymer. Critical micellar concentration (CMC) and amino groups substitute degree (SD %) were found to be 30.3±1.51µg/ml and 21.3±0.58%, respectively. The distinguished peaks of CAP (0.9 and 1.31 ppm) in 1H NMR spectra disappeared, indicating drug loading in the micellar core. Micelles had an average particle size of 163.15 nm and an encapsulation efficiency of 68.45%. The CAP-CS-g-SA was found to be biocompatible in accordance with the hemolysis test. The in vitro release pattern showed 86.78 % in 24 h, indicating the slower release of CAP from micelle, whereas 99.48% CAP was released from non-micellar formulations in 6 h. Conclusion: CAP-CS-g-SA micelle is a promising approach to improve the bioavailability and controlled release of extremely hydrophobic CAP and further in vivo studies would be evident for the treatment of AH using CAP-CS-g-SA.

The influence of the substitution degree and length of alkyl chains on the sizing properties of alkylation starches

In this work, a series of alkylation starches (St-C n) with different alkylation degrees was synthesized by introducing alkyl chains (the number of carbon atoms was 3, 8, and 12, respectively) onto starch. The influence of the substitution degree ( DS) and length of the alkyl chains on the sizing properties of alkylation starches was studied. Fourier transform infrared spectroscopy and proton nuclear magnetic resonance spectra provided evidence for the linkage of alkyl chains onto the starch structure. Benefiting from the flexibility characteristic of the alkyl chain and the weakening hydrogen bonding to starch structure, St-C8 alkylation starch film with a DS of 0.114 exhibited a high elongation break of 4.64%, which is higher than that of the modified starches reported in most of the literature. Moreover, the alkyl chain could reduce the internal stress of the starch adhesive layer among fibers, which improved the adhesion of alkylation starch to cotton fibers. The St-C12 alkylation starch obtained by the longer alkyl chain weakened the adhesion among fibers due to the strong hydrophobic effect. This work provides a new idea to achieve starch plasticization.

Analysis and classification of 1H-NMR spectra by multifractal analysis.

The objective of this research focuses on the development of a statistical methodology able to answer the question of whether variation in the intake of sulfur amino acids (SAA) affects the metabolic process. Traditional approaches, which evaluate specific biomarkers after a series of preprocessing procedures, have been criticized as not being fully informative, as well as inappropriate for translation of methodology. Rather than focusing on particular biomarkers, our proposed methodology involves the multifractal analysis that measures the inhomogeneity of regularity of the proton nuclear magnetic resonance (1H-NMR) spectrum by wavelet-based multifractal spectrum. With two different statistical models (Model-I and Model-II), three different geometric features of the multifractal spectrum of each 1H-NMR spectrum (spectral mode, left slope, and broadness) are employed to evaluate the effect of SAA and discriminate 1H-NMR spectra associated with different treatments. The investigated effects of SAA include group effect (high and low doses of SAA), depletion/repletion effect, and time over data effect. The 1H-NMR spectra analysis outcomes show that group effect is significant for both models. The hourly variation in time and depletion/repletion effects does not show noticeable differences for the three features in Model-I. However, these two effects are significant for the spectral mode feature in Model-II. The 1H-NMR spectra of the SAA low groups exhibit highly regular patterns with more variability than that of the SAA high groups for both models. Moreover, the discriminatory analysis conducted using the support vector machine and the principal components analysis shows that the 1H-NMR spectra of SAA high and low groups can be easily discriminatory for both models, while the spectra of depletion and repletion within these groups are discriminatory for Model-I and Model-II. Therefore, the study outcomes imply that the amount of SAA is important and that SAA intake affects mostly the hourly variation of the metabolic process and the difference between depletion and repletion each day. In conclusion, the proposed multifractal analysis of 1H-NMR spectra provides a novel tool to investigate metabolic processes.

Proton NMR spectroscopy-based metabolomics profiling of doxorubicin-silver nanoparticles for metabolites characterization, and chemical metabolism in breast cancer

In this study, doxorubicin (DOX), silver nanoparticles (AgNPs), and DOX-AgNPs were used to screen metabolome activity in breast cancer (BC) cells. DOX and AgNPs may open an avenue for clinical application and BC metabolic inhibitors; however, their metabolic microenvironmental pathways are not well understood. To evaluate metabolic variations in DOX and AgNPs treated BC cells, proton nuclear magnetic resonance (1H NMR) spectra were coupled with univariate and multivariate statistical methods. The 100 µg/mL of DOX, AgNPs, and DOX-AgNPs-treated BC cells were significantly different from untreated BC cells when multivariate pattern recognition of 1H NMR spectrum data was used. The results show that DOX, AgNPs, and DOX-AgNPs reduced energy, amino acids, neurological, and oxidative stress metabolism. An adenosine monophosphate (AMP), an adenosine diphosphate (ADP), an adenosine triphosphate (ATP), glutathione (GSH), glutamine, glutamate, trimethylamine, and xanthine were all significantly affected. As a results, we propose that DOX, AgNPs, and DOX-AgNPs exposure affected an important metabolic pathway, like pyrimidine metabolism, sucrose metabolism, and glutathione metabolism in BC cells. Data AvailabilityData will be made available on request.

On the 1H NMR spectra of weak electrolytes under the influence of strong electrolytes at low concentrations

Physical chemistry has yet to provide a convincing explanation for the many distinct ways the cosolute's properties are perturbed when under the field of action of salt ions. For that reason, a systematic and gradual approach to the problem was sought, with the present work being a step in that direction. Thus, acetic acid and n-butylamine were selected as simple models for the charged carboxyl and amine groups in more complex solutes, like proteins. The influence of the gradual addition of inorganic salts on these compounds' proton nuclear magnetic resonance spectra was analyzed. The salt concentration varied from 0.01 to roughly 100 mmol.L−1.The reported results suggest that at a low salt concentration (<c.a. 10 mmol.L−1), the effect on the properties of the weak electrolyte results from an indirect action of the salt ions. More specifically, strong electrolytes perturb the auto-dissociation of water whereby H+ or OH– ions are released. Some salts, like NaCl, releasing H+, suppress the dissociation of acetic acid and are neutral to n-butylamine. Other salts, like NaSCN, releasing OH–, shift the reaction of n-butylamine with water towards the reverse direction and are neutral to acetic acid. Moreover, the required quantity of added salt to promote the effects under consideration depends, to a considerable extent, on the valency of the salt ion, the decreasing order of efficacy being as follows: trivalent > divalent > monovalent.Therefore, the experimental facts herein reported show that the effect of salt ions at low concentrations upon the properties of other solutes can be rationalized by conventional chemical concepts, in which chemical equilibrium plays an important role. Furthermore, the results strongly support the classical interpretation of salt ions, which are charged bodies that, in solution, exert chiefly electrostatic forces.

Microemulsion fuel formulation from used cooking oil with carbinol as the dispersion phase

ABSTRACT The current research work investigated the suitability of utilizing Used Cooking Oil (UCO) as a substitute for diesel by using the microemulsification technique. A microemulsion-based biofuel system was formulated using UCO and carbinol as the continuous and dispersed phases, respectively. Winsor type IV stable microemulsion fuel was developed by adding Butan-2-ol as the co-surfactant. The formulated fuel samples were observed to be stable for 30 days. A Phase behavior study was conducted on the samples to analyze the system’s stability, and single-phase emulsions were identified. The particle size of the distributed alcohol phase in the identified system was explored using Dynamic Light Scattering (DLS) study and was found to be 14.6 nm. The results of this work showed the viscosity variation, droplet size distribution, and Proton Nuclear Magnetic Resonance (1HNMR) spectrum of UCO and microemulsion fuel. The optimum blend exhibiting fuel properties under ASTM D6751 standards for biodiesel was 50% UCO, 25% Carbinol, and 25% Butan-2-ol by volume. It gave a kinematic viscosity of 5.74 cSt, a density of 0.862 gm/cm3, and a calorific value of 31.5 mJ/kg. This study recommends using UCO-carbinol-based microemulsion fuels as an effective and economical alternative for the biofuel industry.

Aggregation-Induced Emission-Active Iridium(III) Complexes for Sensing Picric Acid in Water

Herein, two new iridium(III) complexes, namely Ir2 and Ir3, with a phenyl or triphenylamine (TPA) moiety at the 4-position of the phenyl ring at 2-phenylbenzothiazole, have been synthesized, and their emission properties have been studied systematically compared with the non-substituted complex Ir1. These three complexes exhibit aggregation-induced emission (AIE) in H2O/CH3CN. The TPA-substituted complex Ir3 shows the highest AIE activity. All complexes can be used as sensors to detect picric acid (PA) in water. The Stern–Volmer constant (KSV) of Ir3 for the detection of PA was determined to be 1.96 × 106 M−1, with a low limit of detection of 2.52 nM. Proton nuclear magnetic resonance spectra, high-resolution mass spectrometry analysis, and density function theory calculations confirm that the emission quenching mechanism of Ir3 is caused by photo-induced electron transfer. Furthermore, the efficient detection of PA in natural water proves that Ir1–Ir3 can be used as promising sensors in the natural environment. These results suggest that the AIE-active iridium(III) complexes can be used to detect PA under environment-friendly conditions.

Abstract MP26: Lifestyle, Genetic and Epigenetic Factors Associated With Serum Glyca Levels and Results From a Lifestyle Intervention Trial on This Cardiovascular Risk Biomarker

Introduction: GlycA is a novel biomarker of systemic inflammation and cardiovasculardisease (CVD) risk. It is measured by a signal in the proton nuclear magnetic resonance(NMR) spectra (from the N-acetyl methyl groups of N-acetylglucosamine residues).Epidemiological studies have reported associations between GlycA and increased CVD risk.However, there are few investigations examining the link between GlycA levels and lifestylefactors (diet, physical activity (PA), sleep, etc.), gut microbiota, or genetics at the genome-wide level (GWAS); and even fewer studies have analyzed serum GlycA and genome-widemethylation (EWAS) or the effect of lifestyle intervention on the reduction of GlycA.Therefore, our aims were: i) to investigate lifestyle, genetic, and epigenetic factorsassociated with serum GlycA; ii) to examine changes in serum GlycA after 1-y lifestyleintervention in a Mediterranean population. Methods: Cross-sectional and lifestyleintervention analyses were undertaken in a Mediterranean population at highcardiovascular risk (n=426 older subjects with metabolic syndrome in the PREDIMED-Plus-Valencia trial; ISRCTN89898870). Lifestyle variables were assessed by validatedquestionnaire and quantile-g-computation methods were used to analyze their jointcontribution. Serum GlycA was measured by NMR spectroscopy. Genome-wide genotypingand DNA-methylation were determined by Illumina arrays (OmniExpress and EPIC).Exploratory omics-wide and targeted analyses on GlycA (focusing on autophagy genes andmicrobiome-host-related genes) were undertaken. Changes in serum GlycA levels after a 1-y lifestyle intervention (intensive intervention group with Mediterranean diet and PA versusthe control group) were assessed in a subset of participants. Results: GlycA levels atbaseline (Mean: 1.49+/-0.20 mmol/L) were significantly associated with branched-chainamino acids and a highly atherogenic lipid profile. Also, we obtained an association withdietary factors and PA. Omics analysis suggested novel SNPs (in SFMBT2- DAB1 and TEK)and methylation sites (CpG in RAD50, PPP1R9B, ZDHHC4 and LSP1) associated with GlycA. We also obtained associations with host-microbiome related SNPs in FUT2 and withmethylation signals in selected autophagy genes (STX7, TAX1BP1, ATG9B and ATG10).Moreover, in the intervention trial we detected a significant (P&lt;0.05) decrease in the GlycAlevels after 1 y of intensive lifestyle intervention in comparison with the control group. Conclusions: Serum GlycA levels were strongly associated with cardiometabolic risk factorsin this Mediterranean population and linked to lifestyle variables. Additionally, we haveidentified some genetic and epigenetic factors related to GlycA that may modulate theselevels.

Synthesis of high hydroxyl value polyol from rubber seed oil by using Na2WO4/H3PO4/H2O2‐based catalyst complex formed in aqueous phase

AbstractVery high acid value rubber seed oil (RSO) and low acid value esterified rubber seed oil (RSOE) were used to synthesize high hydroxyl polyols in a one‐pot two‐temperature stage reaction. The Fourier transform infrared spectra and proton nuclear magnetic resonance spectra demonstrated the presence of hydroxyl groups in the polyols. By optimizing the influence of H2O2 content and technological conditions such as hydroxylation temperature, pre‐reaction time, and hydroxylation time, a suitable technological process for polyolization was found for each oil. With the same pre‐reaction time (20 min) and hydroxylation time (2 h), 100°C was the suitable temperature for RSOE polyolization and 110°C for RSO. Due to the very high acid value of RSO, the appropriate H2O2 content for its polyolization (DB (double bond)/H2O2 ratio of 1/1.75) needed to be larger than that for RSOE polyolization (DB/H2O2 ratio of 1/1.5). The catalytic selectivity in RSOE polyolization was very high (0.91), so the hydroxyl value of the RSOE polyol reached 500 mgKOH/g while it was only 393 mgKOH/g with RSO polyol.